Method and means for compounding flame and waterproofing compositions for aqueous cellulosic media



Patented May 1935 UNITED STATE METHOD AND Mantis FLAME orrlce' 'ron 'coiuronnnnvc poration of Delaware Application March 23, 1e33, @2391;

n This invention concerns the, fiame and, whe proofing of aqueous cell-ulosic media and .to a' composition .0! matter'i therefor together with themethodoimakingthesame'.

,As pointed out copending application 651,363, filed January-l2, 1933 ior Flam'e -prooiing composition oi matter andjprocesst-for making the same, it, has heretofore been considered commercially impossible to render aqueous cell'ulosic media both fiame and water-proof. If the water-proofing compound was applied first its efiectiveness was destroyed by,the application oi the flame-proofing'composition, and vice versa,

and in addition there was no single composition known which would rendersuch media. both flame and water-proof. Y

One of the objects of the present invention is to overcome the above mutually destructive'eiiects of utilizing separate mutually hostile-flame 'and water-proofing compositions and to-provide a single composition which will accomplish'both results effectively and practicably Another object of my invention resides in the method of compounding a single composition (which will render aqueous cellulosic media both fiaine and water-proof as well as a method for making such composition. Y

'A further object resides in compoundingcertain relative quantities under controlled cinditions. 7

A still further object resides in the proces and arrangement of apparatus for compounding certain specified constituents in certain relative proportions under controlled conditions in a certain 85 order and in applying the same to the medium so as to secure the greatest effect therefrom.

Other and further objects and advantages will be understood by those skilled in the art or will 7 be apparent or will be pointed out hereinafter.

In the accompanying drawing the figure illustrates a more or less schematic arrangement for compounding the composition ofnnatter and for applying it to the medium as will-be hereinafter more fully described.

In the upper left-hand corner of the figure of the drawing are a number of containers or vessels in which I preliminarily provide the various solutions from which the present composition of matter maybe made. Reading from left to 0 right these containers are'designated to'contain alum solution, boric acid solution, ammonium carbonate solution, ammonium sulphate solution,"

aqueous colloid solution, ammonium chloride solution, boric acid solution, bor'ax solution, and

v 5 soap solution. It is to be understood at the outand, asshown these discharge pipes lead to a set that this arrangement is variable according to circumstances; but'in generaIJtIie solutions are more or lessso arrangedin the receptacles that certain groups of them can be discharged into common oi'ipredetermined receptacles or tanks. Asshown each solution container I0 is provided with a lower discharge pipe ll, each such discharge pipe being provided with a suitable valve l2 for'opening or'closing the pipe II or for controlling the rate of fiow therethrough. It will be noted that the aqueous colloid solution container has two such dischar'gepipes as it may be desired to discharge part of the solution into dferent tanks or iflsuch is not the case, either pipe ll may be used while the other is shut oil. As shown in the drawing further these discharge pipes II are so directed as to discharge intoa selected one of a number of tanks indicated by the, numeral I3, two such tanks being shown although any required or desired number may be used. Each such tank I; is provided with a suitable temperature indicating device I l and with any necessary or desired gauge member l5. Predetermined amountsirom predetermined receptacles are? discharged into the;seiected tank l3 as will hereinafter more in detail be pointed out. 1 K

Each of tanks l3 in turn is provided with a dischargel6 having a suitable valve l'l therein,

larger mixing tank |8,-likewise provided with a temperature indicating device I 9. In this tank the final composition is brought to condition and from such tank the composition when finished may either be directed directly to the treating tank 24, or if a succeeding portion of material is being finished in tank 18, previously completed composition may in the meanwhile be heldin intermediate tank 2|, also provided with a temperature indicating device 22, and from which tank the finished solution can be fed as needed to treating tank 24 by way of suitable pipes and valves as will be understood.

The method schematically outlined above comprises in detail the following steps and operations substantially in the order named except as otherwise pointed out.

First, for example, I heat five gallons or we. to about F. and to the same I add in the order named 48 ounces of ammonium sulphate, 50 16 ounces of ammonium carbonate, 20 ounces of boric acid and 16 ounces of borax. Upon adding the ammonium, sulphate, stirrlng'is carried out toensure complete dissolution thereofin the water. The ammonium carbonate is 'addedincreat mentally under constant I add under con stirring, care being taken to prevent violent efiervescence which may oc The boric acid previously dissolved in one gallo 'of boiling water is not added until ef-. fervescence has ceased, and, after thoroughlyadmixing these three, the borax is then added and thoroughly mixedby, stirring or the like. Next, stant stirring to the foregoing, 1.6 ounces of starch such asarrow-root starch which has been previously cooked to about 1 Baum. I then dissolve6 ounces of anysuitable soap in one gallon of water .and bring thisup to the boiling point by heating, whereupon it is added to the foregoing ingredients. An emulsiflcation takes place upon ,the addition of the soap solution and when complete emulslflcation and. dissolve therein five 4 ion of water to t is dissolved and additionally for ,a perio one constant stirring.

has tak n place the temperature is reduced'to about 11 F. and the composition digested for two hourshthereby forming a first composition.

I heat five gallons of water to the boiling point pounds of ammonium ric acid and one pound named, and each succhloride, 3 pounds or be of borax in the orderceeding material is added only after the preced- I and 2 gallons of water and heat to 200 F. under constant stirring, to which 400 c. c. of glycerin or its equivalent may be. added if a flexible medium is desired. I thoroughly stir the gelatin solution and then. mix it with the ammonium chloride-boric acid-borax solution under con stant stirring for about thirty minutes and then the same is digested for about one hour at about 140 F.; I dissolve 3 ounces of any suitable soap. such as sodium resinate, stearic acid or sodium stearate, in one gallon of water, heat to the boiling point and add 8 ounces of dextrine, stirring such'constantly to ensure, uniformity,'and then, adding such to the ammonium chloride-bone acid-borair-gelatin solution, thereby f rming a second composition.

To form my third composition I heat one galhe boiling point and add thereto 15 ounces of soap if necessary the'solution is filtered to remove undissolved matter. 1 To form my fourth composition I dissolve 32 yneutral alum-in 2 ounces of alumpreferabl gallons of cold water. Eaeh of these four compositions are digested d of about four hours, stirring occasionally or from time to time to prevent the settling out at the bottom of colloidal matter. After each of the'four compositions is thus come pounded and treated-I finally combine. them in a common vesseLin the order one, 'two, four, three. In other words, the first two compositions-are added in order to the vessel and then the fourth composition is added, the third composition being reserved until last and'being added under vigor- If the ingredients of the above-mentioned compositions are designated or expressed as parts, since one gallon fluidmeasure is equivalent to 128, fluid ounces, and one pound avoirdupois is equivalent to 16 avoirdupoi's ounces, and one cubic centimeter is equivalent to .03381 fluid ounces, by

way of example, the flrst,c omposition includes '640'parts'of water at 120 F. to which is added 48 parts of ammonium sulphate, 16,parts of ammonium carbonate, 20 parts -of boric acid, and 16 parts of borax. The boric acid is previously dissolved in 128 parts of water. 16 parts of starch bark (tannin). The soap bark are added and 6 parts of water. 7 In the second composition, the 5 gallons of water may be designated as 640 parts, the 5 pounds-of ammonium chloride as 80 parts, the 3 7 v5 pounds of boric acid as 48 parts, the 1 pound of borax as 16 parts, the 2 pounds of solid gelatine as 32 parts, the 2 gallons of water as 256 parts, L 400 me. of glycerine as 13% parts, the 3 ounces of suitablesoap-asii parts, the 1 gallon of water as 10 128 parts, and-the 8 olmces of dextrine as 8 parts. In the third composition, the 1 gallon of water r may be represented as 12&parts and the 15 ounces of soap bark as 15 parts.

In the fourth composition, alum may be repre-, sented as 32 parts and the whterzas 256 parts. It should be noted that when I refer to a fluid such as water as including so many parts, that I have reference to fluid parts, and further, when referring to a substance suchas alum, soap, etc., that I refer to avolrdupoisparts.

In certain cases-where it is impractical or'inconvenient I mayu nodify the above method by dissolving each constituent ab parts of soap are dissolved in 128 res and under the proper conditions above set forth before being-used.

- In applying the composition of the present invention to the medium to be flame and waterproofed, 'it may be any suitable aqueous cellulosic medium or any suitable textile or fabric material or an equivalent or derivative thereof, I proceed in a typical case as shown in the right-hand por-' tion of the figure of the drawing. A suitable roll of the material to be treated i 30 isrevolubly mounted as on a roller 3| journalled instandarda 32 whereby the material can be readily unrolled. It passes first by way of suitably constructed idler and/or tension rolls 33 through the treating tank 24 to which is fed my present composition of matter as will be understood. from the drawing. The length of the tank is such that the material will be subjected to the comp length of timemfter which the material emerges from thetank and passes more or less vertically upwardly. between the rollers 34 which act as J- squeeze rollers thus eliminating excefi composition from the materials These squeeze rollers may 5 I on to the treating tank 24 that the excess composition may eithendrop back to the tank or be otherwise collected and saved for re-use. From squeeze rollers 34. the material then passes through tension rollers 35 whence it is guided as by means of short endless belts 36 mounted on rollers 31 into" the interior orvaporizing chamber -3 8 of treating er 60. Belts 36 may be synchronized perforated rubber belts and the right hand set of rolls may be perforated, hollow, andconnected to a vacuum or suction connected as hereinafter pointed out in .connection with members 40 and 4|. e

In vaporizing chamber 38 air, heated or otherwise, is-caused to pass over, through and around the treated material so as to eifect ahnost instantaneous vaporization of excess composition andto complete a substantial drying of the material. I Such vaporizing air may be suitably generated as by a supply blower or fan 6| which creates a blast 11s 39 mounted in the exit rizing chamber the material is y way of guide ro side of the vapo osition for the desired caused to passover a rubber perforated belt 40 mounted in endless fashion on'the rolls 4|. One of suchrolls 4| is shown as hollow'and provided with perforations 42 and connected to this hollow roll by means of a suitable connecting pipe 43 is an exhaust or vacuum pump or fan 44 which results in a sucking of air through the rubber perforated belt 40, thus holding the material in contact with the rubber belt, and, further drying the material which may be additionally assisted by a hood 64 of frusto-conical-shape connected into conduit 62 and having, if desired, a thermostatically controlled stem or electrical means for warming or heating the air passing through said hood. As shown such is represented by an electrical resistance coil 65 and it is clear that the hood itself directs air onto the rubber belt and the mediuzn thereon. Roller 45 may be provided for any suitable purpose such as maintaining close contact between the various elements at the perforated roll. While the rubber belt and its rolls have been shown as located within a chamber 46, this chamber may or may not be used and is only I illustrative.

' a I may makesuitable or desired modifications, sub- From the perforated roll the material passes by way of suitable idler 'or guide rolls 41 to a festooning machine indicated by the numeral 46 and consisting mainly of a framework having cross bars 49 on which are journalled suitable rolls 50, so that the material passing therethrough can be given a relatively long and tortuous path for completing the drying and for therefore, disclosed a single tcom'position of mat-.

ter which consists of a ni'orebr less complex solution together with a meansx'for making the same which is adapted efiiciently to render media of. the nature explained .both flame and water-proof at one and the 'sametime. Upon compounding such a composition and then ap-' plying it to the medium or material to be flame and water-proofed and then 'drying the same.

after the application of the composition, 1 findthat I can accomplish in a single and relatively simple process a finished commercial article which is non-flammable and water-proof.

It is clear that the above is intended more in an illustrative than in a limitative manner and stitutio additions or omissions without departing from the spirit and scope of the iIlVEIl-e tion, particularly as designed by the subjoined claims. to the precise constituents set forth, but'such is on the contrary subject to some considerable variation. In a particulancase constituents are chosen which will have the desired effect lunch the particular medium and which will contain nothing deleterious to that medium which, in-

cidentally, has been one of the serious diiflculties with previously contemplated compositions. I may also in similar, manner vary the concentrations or amounts of the constituents depending again upon the particular medium being treated andthe degree of resistance to flame and water which is to be imparted. Other and further variations will be understood by those familiar with the compounding of chemicals and the treating of various media therewith.

In setting forth the foregoing it is further to be understood that where I specify certain chemicals I am not limited to precisely such but I thereby intend to include their equivalents or substitutes, capable of producing the intended results.

What I claim as new and desire to secure by Letters Patent is:

1. A method of flame and water-proofing aqueous cellulose media comprising carrying out the following steps in substantially therelative proportions indicated as follows: heating 640 parts of water to 120 F., adding 48 parts of ammonium sulphate and stirring until completely.

pounded materials, bringing about emulsiflcation I of the whole, and then,- lowering the temperature to about 110 F. and digesting for about 2 hours, thereby forming a first composition:

bringing 640 parts of water to the boiling point and dissolving therein 80 parts of ammonium chloride, 48 parts of boric acid and 16 parts of bor'ax in the order named and each after the preceding .has been completely dissolved, stirring the same thoroughly after all three have been added and dissolved, separately dissolving 32' parts of soft gelatine in 256' parts of water and heating to about 200 F. under constant stirring, and thereafter, optionally adding thereto 13 /2 parts of glycerine, stirring thoroughly, and then, adding the same to the ammonium'chloride boric acid-borax solution under constant stirring for about 30 minutes, and then digesting for about one hour at about 140 F. dissolving 3 parts of suitable soap in 128 parts of water, heating to'boiling and adding 8 parts of dextrine,

stirring such constantly to ensure uniformity and then adding such to the ammonium chlorideboric acid-borax-gelatine solution, thereby forming a second composition; bringing 128 parts of water to the boiling point, dissolvingtherein 15 digesting each of the four compositions for about 4 hours while stirring from time to time; com- 1 bining the first, second and fourth compositions For example, I am not strictly limited" in a common vessel\ and then adding the third 2. A method of compounding a composition of matter for flame and water-proofing aqueous celparts of soap bark and filtering, thereby forming lulose media and their derivatives comprising heating 640 parts of water to 120 F., adding 48 partspLammonium sulphate and stirring until completely" dissolved, adding 1.6 parts of ammonium carbonate incrementally under constant stirring until efiervescence ceases, adding 20 parts of boric acid previously dissolved in 128 parts of boiling water, adding 16 parts of borax and thoroughly mixing, adding 16 parts of starch previously cooked to about 1 Baum and thoroughly mixing in the same'under constant stirring; dissolving 6 parts of suitable soap in 128 parts of water and bringing it to the boiling point, thereafter adding the same to the previously compounded materials, bringing about emulsification of the whole and then lowering the temperature to about 110 F. and. digesting for about 2 hours thereby forming a first composition; bringing 640 parts of water to the boiling point and dissolving therein 80 parts of ammonium chloride, 48 parts of boric acid and 16 parts of bora r in the order named, and each after the preceding has been completely dissolved, stirring the same thoroughly after all three have been added and dissolved, separately dissolving 32 parts of soft gelatine in 256 parts of water and heating to about 200 F. under constant stirring and thereafterpptionally adding thereto 13 /2 parts of glycerine, stirring thoroughly and then aooama adding the same to the ammonium chlorideboric acid-borax solution ring for about 30 minutes and then digesting for about one hour at about 140 F.; dissolving 3 parts of suitable soap in 128 parts of water, heat- Q ing to boiling and adding 8 parts of dextrine, stirring such constantly to ensure uniformity and then 'adding such to the ammonium chlorideboric acid-borax-gelatine solution, thereby forming a second composition; bringing 128 parts of water to the boiling point, dissolving therein 15 parts of soap bark and filtering, thereby forming a third composition; dissolving 32 parts of alum in 256 parts of water as a fourth composition; digesting each of the four compositions for about 4 hours while stirring from time to time; combining the first, second and fourth compositions in a common vessel and then adding the third composition under vigorous stirring.

FREDERICK W. HOCHSTETTER.

under constant stir- 

